Tungsten-titanic target formagnetron sputtering and method of its receiving

SUBSTANCE: it is implemented deep vacuum refinement by multiple remelting of tungsten and titanium with receiving of polycrystalline ingots of titanium and tungsten monocrystal. Then from the polycrystalline ingot of titanium it is manufactured disk, in which in diffusing area per two concentric circles alternate there are bored holes and by press fit there are fixed in it cast cylindrical inserts from tungsten monocrystal, preliminarily subject to grinding and cutting per exact lengths. Target, recived by mentioned method, consists of cast disk made of high-clean titanium and cast cylindrical inserts made of high-clean monocrystalline tungsten, located in diffusing area of disk by two concentric circles alternate. Additionally area ratio on surface of target, taken up by tungsten and titanium, provides receiving of films at magnetron sputtering composition 35-40 wt % of titanium, tungsten is the rest.

The invention relates to the production of atomized metal targets for microelectronics. In the production technology of silicon very large scale integrated circuits (VLSI), alloys of tungsten and titanium are used as diffusion barrier layers between the silicon substrate and the metallization of aluminum alloys. Tungsten-titanium thin film barriers are made by spraying a tungsten-titanium target. Such targets are produced by mixing the original powders of tungsten and titanium, followed by heating and pressing.

Closest to the claimed object is U.S. patent No. 5896553 from 20.04.1999 (prototype), which describes a single-phase tungsten-titanium sputtered target and method of manufacture, which consists in mixing powders of tungsten and titanium and pressing at a temperature, pressure and time sufficient to achieve a mutual solid solution of tungsten and titanium with the formation of the beta phase. The disadvantages of the prototype include the following:

- The product obtained from the complex operations including extrusion and annealing the mixture of powder materials, which may result in saving or making uncontrolled impurities, including carbon, oxygen and nitrogen, i.e. the impurity composition of the target defined by the manufacturing method.

- Don is but the achievement of the minimum porosity of the target material.
Produced according to the description of the target has a specific density, comprising 90-95% of theoretical, as a result, when the operation is observed instability of the dispersion, swelling of the target due to outgassing from the volume and the formation of columnar microstructure in sputtered tungsten-titanium films.

- Getting-phase targets the beta-phase is difficult to achieve. In the manufacture of sprayed tungsten-titanium target, due to the passing of mutual diffusion processes, the balance in real time not is never, therefore, tungsten and titanium are unevenly spaced, the microstructure of multiphase and it has a negative impact on the quality of the deposited barrier layers.

- The use of high pressure (up to 40 kpsi) in combination with high temperatures (up to 1650°C) in inert gas or vacuum within 3-6 hours leads to extraordinary hardware and process more complicated and expensive the whole process of production targets.

Technical problem - improving the quality and reliability of barrier layers of a tungsten-titanium alloy through the use of targets for magnetron sputtering, obtained by vacuum metallurgy. In this case, the dispersion is subjected alloy target with a specific density of 100%, do not have the disadvantages of metal-ceramic Mish is yum.
Process variants can be the use of a target made of cast blocks of high-purity tungsten and titanium, or simultaneous sputtering (co-sputtering) two cast targets of tungsten and titanium of high purity. The latter case is the interesting possibility of obtaining a tungsten-titanium films of any composition by choosing the rate and deposition time for each metal. This method used by the authors for testing regimes for the films with optimal electrophysical parameters. The desire to maximize the purity of the starting materials of the targets has led to the design of a composite target. Used the results obtained by the authors in a co-sputtering two cast targets. Composite tungsten-titanium target is a flat base made of high-purity titanium with cylindrical inserts of single-crystal tungsten of high purity. For the manufacture of titanium ingots used dual electron-beam remelting in a high vacuum, the single crystals of tungsten were obtained by electron-beam zone melting in a high vacuum refining for several liquid passes molten zone. On the titanium disc made of polycrystalline ingot, in the spray zone (zone erosion) in two concentric okrujno the holes in staggered drilled holes,
which zapressovyvat tungsten cylindrical insert brushed in diameter and cut to length in the sheet.

Figure 1 presents a General view of a composite target for implementing the inventive method: 1 - titanium disk, 2 - insertion of a single crystal in the amount of 56 pieces. Tungsten inserts the specified diameter and number were placed so that the sprayed surface of the target in the area of the erosion area ratio plots of tungsten and titanium corresponded to the desired value in the tungsten-titanium films.

An EXAMPLE IMPLEMENTATION of the METHOD

Implementation options for a tungsten-titanium films with a given ratio of components co-sputtering two targets was performed to determine the optimal modes of atomization and the optimum ratio of the elements in the diffusion barrier layer, when there is the least mutual solubility on the border with aluminum metallization, is a high resistance layer in combination with a low specific resistivity, good adhesion and optimum mechanical properties of the barrier layer. Target, which is a flat disk with a diameter of 78 mm, made of polycrystalline ingots of high-purity titanium and tungsten. The deposition of the films was carried out on the installation magnetron raspy is possible with separate magnetrons.
The experiments showed that the rate of deposition of both metals to be linearly dependent on the discharge power. In experiments determined the capacity of spraying each of the two targets required to obtain a tungsten-titanium film with a specified ratio of tungsten/titanium. To assess the quality of deposited films on the value of the surface resistance and the thickness of the films measured resistivity. Figure 2 presents the dependence of the electrical resistivity of the films on the ratio of titanium and tungsten (figure 2, point a, 1, 2, 3, 4, 5, 6, In). When applied to the same or similar conditions, the tungsten-titanium layer by sputtering metal-ceramic target, obtained by powder metallurgy using a high-purity source powders and with the exception of depositing contaminants on the stages of manufacture of the target, the specific resistivity was 130 µohm. cm (figure 2, point C). In films of the same composition produced by co-sputtering two cast targets of high-purity tungsten and titanium, the specific resistivity was 62 µohm. cm (figure 2, point (E), i.e. two times lower.

It should be noted structural features of the films obtained by spray powder and cast targets. Powder targets can be sprayed only at a low power (<1 kW) following the journey of the gas release and swelling in the warm-up target up to 300°C. in the sputtering process.
Figure 3 presents a schematic cross-section system with barrier tungsten-titanium layer. At low speeds there is formed a columnar structure. Pores decorate the borders of the columns (crystallites), consisting of a dense core (matrix W(110) with micro inclusions of titanium), surrounded by a less dense, porous material. This structure dramatically reduces the barrier properties of the film after annealing the tungsten diffuses into the aluminum with the formation of WAl12and aluminum - tungsten-titanium film with the formation of TiAl3. The cast of the target was sprayed at high speeds (power >3 kW), while the gas release and swelling does not occur, and the microstructure of the films is characterized by a high dispersion with a grain size of 10-20 nm.

Based on the results obtained by co-sputtering two targets, proposed a composite target (figure 4), subjected to the tests to study the reproducibility of the composition and properties of tungsten-titanium films. 4 shows a composite target and new target b target produced by 20%. The sputtering was performed in an industrial setting "Oratorio-5" in argon. The rate of deposition of films of 1.8±0.1 nm. with-1. Film besieged on a silicon wafer, pre-heated to 250°C. the film Thickness of 0.18±0.02 mm, the specific resistivity is less than 5 Ω/□. Controlled composition, the article is alternia features,
the reproducibility of the depth of the layer, electrophysical parameters. Spectral analysis showed that the composition of the films done by sputtering a composite target at various stages of its operation (in particular, in the initial period and after 145 cycles spraying when there is erosion of the spray zone) corresponds to a content of titanium 35 to 40 at.%, the rest of the tungsten. Deviation from this ratio during the operation of the target does not exceed 2-3%. The specific resistivity of the films was at 60-70 µohm. cm (figure 2, point E). So, the proposed target is designed so that it sprayed surface has a ratio of areas occupied by titanium and tungsten, providing a tungsten-titanium films of the desired ratio, namely 35 to 40 at.% titanium, the remainder tungsten.

1. Method for the production of tungsten-titanium target for sputtering, comprising deep vacuum refining multiple remelting of tungsten and titanium with obtaining polycrystalline titanium ingot of single crystal tungsten, production of polycrystalline ingot of the titanium disk, in which the sprayed area on two concentric circles in a checkerboard pattern drill holes and press fit attached to them cast cylindrical insertion of single crystals in which iframe,
pre subjected to grinding and cutting to length.

2. Tungsten-titanium target for sputtering, characterized in that it is obtained by the method according to claim 1 and consists of a molded disc of high-purity titanium and cast cylindrical inserts of high-purity single-crystal tungsten, located in the spray zone of the disk by two concentric circles in a checkerboard pattern.

3. The target according to claim 2, characterized in that the ratio of the areas on the target surface occupied by tungsten and titanium, provides the film with magnetron sputtering composition of 35 to 40 at.% titanium, the remainder tungsten.

SUBSTANCE: invention concerns electric vacuum ultra high frequency devices, particularly in O-type traveling wave lamp with magnetic periodic focusing system (MPFS). Lamp includes MPFS combined with resonance slow-down system and consisting of intermittent axially magnetised ring magnets, polar headpieces and ferromagnetic inserts. To achieve required harmonic component level in magnetic field with non-sinusoid distribution, at least a part of MPFS behind high frequency power input consists of adjoining cells, each including at least one unidirectional magnetisation magnet and three ferromagnetic inserts between polar headpieces. Magnets in each two neighbour cells have opposite magnetisation. Inserts are positioned with gaps against polar headpieces in hubs in the form of step rotation bodies and fixated by annular elements, and form inner cavities of high frequency resonators in slow-down system. Hubs and annular elements are made of non-magnetic material with high heat conductivity and comprise vacuum shell together with polar headpieces.

EFFECT: enhanced current permission of beam in high-performance traveling wave lamp in short-wave part of UHF range due to intense electron stream focusing in transit channel.

SUBSTANCE: invention concerns electric vacuum ultra high frequency (UHF) instruments, particularly construction of O-type traveling wave lamp with magnetic periodic focusing system (MPFS). Lamp includes MPFS combined with resonance slow-down system and consisting of intermittent axially magnetised ring magnets, polar headpieces with ferromagnetic hubs and non-magnetic diaphragms with capacitance bushings, positioned between them and forming transit channel. At least a part of MPFS behind high frequency power input includes ferromagnetic insert forming slow-down system resonators together with adjoining polar heads. Another resonator part is formed by diaphragm in the form of step rotation body, and annular element fixating the insert in diaphragm. Diaphragms and annular elements are made of non-magnetic material with high heat conductivity. Selection of ferromagnetic insert profile, size and position between polar heads defines magnetic field with given high harmonic components and non-sinusoid distribution.

EFFECT: enhanced current permission of beam in high-performance traveling wave lamp in short-wave part of UHF range due to intense electron stream focusing in transit channel of traveling wave lamp with low pulsation.

SUBSTANCE: tight block switching fixtures represent welded components with separate tight leadouts incorporating rigid conducting terminal extenders with a flat flange while coaxial tight leadouts incorporate flexible terminal extenders fitted on the rods arranged on the surface of ceramic plates in rows with the difference in height of top points of the flexible conducting terminal extenders between the first and every subsequent row h defined from the formula h=l·sinα, where l is the distance between the first and each subsequent row and α is the angle of inclination of a plane of the contact between the top points of the aforesaid flexible conducting terminal extenders to the ceramic plate plane. The terminal block comprises also cylindrical extender sleeves with tabs arranged on both end faces. Note that the said tabs of the lower end face are bent along the radius by the angle of 90° outward from the sleeve axis of symmetry. Note also that, at the top end face, the said tabs are vent two times by 90° towards the aforesaid axis of symmetry of the sleeve. To weld the aforesaid fixtures, a pulsed laser radiation makes a heating source.

EFFECT: high level of technological and operational properties of proposed tight block.

SUBSTANCE: slow-wave system of spiral type is suggested, which contains two hollow cylinders made of aluminium nitride with wall thickness of smaller hollow cylinder of 0.3÷1 mm, and installed one inside another with the possibility of mutual contact provision along the whole surface of their contact, metal spiral made by laser beam on the external surface of smaller hollow cylinder, at that height of metal spiral section in the plane that is perpendicular to its length is provided as at least 0.05 mm. At that internal diameter of smaller hollow diameter, length of metal spiral, distance between its turns and external diameter of larger hollow cylinder are determined by wave length and value of maximum output power of electronic SHF appliance.

SUBSTANCE: slow-wave system of spiral type is suggested, which contains two hollow cylinders made of aluminium nitride with wall thickness of smaller hollow cylinder of 0.3÷1 mm, and installed one inside another with the possibility of mutual contact provision along the whole surface of their contact, metal spiral made by laser beam on the external surface of smaller hollow cylinder, at that height of metal spiral section in the plane that is perpendicular to its length is provided as at least 0.05 mm. At that internal diameter of smaller hollow diameter, length of metal spiral, distance between its turns and external diameter of larger hollow cylinder are determined by wave length and value of maximum output power of electronic SHF appliance.

SUBSTANCE: invention relates to electronic technology, in particular to multi-beam electron guns for powerful multi-beam electro-vacuum microwave devices of O-type, for example, for powerful pulse multi-beam klystrons and TWT. The multi-beam electronic gun contains ring cathodes fixed in the general cartridge clip, electronically isolated from them in the form of a plane-parallel metallic plate with apertures and an anode with apertures. Each of the ring cathodes contains an internal ring core and its coaxially to surrounding ring emitter with a concave spherical emitting surface, turned to the side of the anode. The internal ring core on the side facing the anode has a ledge in the form of the hollow cylinder and the ring groove surrounding it, located coaxially internal ring core. The end of a protrusion is rounded and the apex of the protrusion is combined with a plane, passing through the edge nearest to the controlling electrode of the spherical emitting surface of the ring emitter, the internal diameter of the protrusion is equal to internal diameter of the internal ring core, the external diameter of the protrusion is equal to internal diameter of the ring groove, the external diameter of the internal ring core is equal to the internal diameter of the ring emitter, thus distance H from the base of the groove to the top of the protrusion, the external diameter D2 of the protrusion, the rounded radius R of the protrusion, the external diameter D3 of a ring groove are determined by the set conditions.

EFFECT: simplification of the design of a multi-beam electron gun, increase in the dielectric strength, stability and reliability of its work in powerful pulse multi-beam devices of short-wave area of the microwave band.

SUBSTANCE: invention is related to electronic microwave equipment, namely to powerful wide band microwave devices of O-type, for instance, to multiple-beam klystrons that mostly operate in medium and short-wave part of centimeter range of waves length. Microwave device of O-type consists of sequentially installed along its axis electron gun, active resonators in the form of wave conductors segment and collector. Active resonators are made as stepwise changing in height, where height is the distance along microwave device axis between end walls of active resonator. In active resonator floating-drift tubes are installed linearly in rows and are fixed in its opposite end walls, and ends of coaxially installed floating-drift tubes are separated by permanent high-frequency gap. Central rows of floating-drift tubes are installed in sections of active resonators with the least height, and subsequent rows of floating-drift tubes that are installed along both sides of central rows, are installed in sections of active resonators with higher heights. It is also suggested to use inlet and outlet active resonator with non-symmetric installation of floating-drift tubes relative to opposite side walls of these resonators. Inlet active resonator may be connected to energy input directly through inlet wave conductor or through inlet passive resonator and inlet wave conductor. Outlet active resonator may be connected with energy output directly through outlet wave conductor or through one or several outlet passive resonators and outlet wave conductor.

EFFECT: increase of efficiency factor at the account of improvement of electric field distribution uniformity in the sphere of electronic flow interaction with microwave field.

SUBSTANCE: multi-section collector of electric vacuum device with recuperation is suggested, made in the form of hollow cone. Hollow cone is made monolithic from aluminium nitride by method of hot-pressing, metal closed conductors are made by means of laser beam scanning of external surface of hollow cone in points of their corresponding installation at the depth that is equal to hollow cone thickness. At that thickness of hollow cone and width of metal closed conductors are determined by output parameters of electric vacuum device.

EFFECT: increase of output power and efficiency factor; increase of reliability, durability and manufacturability.

SUBSTANCE: invention is related to the sphere of electrodynamics and may be used for creation of multiple-frequency generator of microwave oscillations, for example, on the basis of traveling-wave (TWL) or backward-wave (BWL) lamps. Non-uniform delay-line system in the form of joined resonators chain constitutes wave guide, which is baffled with flat membranes that are perpendicular to system axis and contain coupling slots and channels for electrons transit. Resonators chain is divided in sections. Geometric dimensions of membrane coupling slots in every section of resonators are selected in such a way so that pass band of each subsequent section is more than the previous one, at that top limit frequencies of pass bands of every section are same. Turndown of delay coefficient in frequency band of every section should not exceed turndown of delay coefficient of the last section. Selection of required pass band and dispersive dependence is achieved by alteration of geometric dimensions of toroidal resonators.

EFFECT: increases coupling impedance along the length of delay-line system at selected frequencies in preset frequency band.

FIELD: high-frequency electronics; devices for protecting microwave radio receivers of radar stations against heavy power fluctuations in superhigh and extremely-high frequency bands.

SUBSTANCE: proposed device has electron gun, input and output electrodynamic structures unidirectionally coupled through electron flow and separated by means of diaphragm with hole to pass electron flow, as well as collector. Homogeneous magnetic field is oriented to electron flow direction. Each electrodynamic structure is formed by electromagnetically coupled and series-connected resonators. Unidirectional coupling of electrodynamic structures through electron flow is provided only between resonators of these structures closest to each other and diaphragm is disposed in-between.

SUBSTANCE: it is implemented aluminium reactionary evaporation and reactionary gas is fed into coating spraying machine on belt padding with receiving of coating from aluminium oxide. Before plating made of aluminium oxide on padding by magnetron sputtering it is applied short close layer of metal or metal oxide.

EFFECT: there are received transparent barrier coatings without high technological expenditures.

SUBSTANCE: zone of device for application of coatings consists of at least two compartments, the first of which contains the first target, and the second one - the second target. In the first coating layer is applied in metal mode, which consists in the fact that the first target is used and metal layer is applied in atmosphere of gas that does not enter into reaction. In the second compartment layer is applied in transitional mode, which consists in the fact that the second target is used and layer of target material oxide is applied in atmosphere of gas that does not enter into reaction and chemically active gas with the rate slower than the rate of coating layer application in metal mode, or layer is applied in oxide mode, which consist in the fact that the second target is used and layer of target material oxide is applied in atmosphere of gas that does not enter into reaction and chemically active gas with the rate slower than the rate of coating application in transitional mode. Layer of coating in transitional mode or oxide mode is applied with the second target from material with value of free Gibbs energy ΔG, which is equal or less than - 160 kcal/mole O2, or for the second target during application of layers in transitional mode and oxide mode material is used with the difference between its ΔG and ΔG of the first target material used during application of coating in metal mode of at least 60 kcal/mole O2.

EFFECT: reduction of total number of zones for application of coatings.

SUBSTANCE: method includes actuation gas feed into evacuated vessel, pulsed lasing of plasma stream and high-energy ion beam and its alternate action to support in distance. Discrete plasma stream is created by means of firing of high-current high-voltage diffusive discharge which is formed by means of passing through stationary plasma of magnetron discharge of current pulse duration 10-6...1 s, density 0.3-100 A/sm2 and repetition rate till 103 Hz. Specified distance is chosen more than time of plasma recombination of high-current high-voltage diffusive discharge in volume of evacuated capsule. Effect to support by pulsed beam of high-energy ions is implemented with energy which is not more than 106 eV and with repetition rate till 103 Hz. At that it is implemented rejection of high-voltage fault of accelerating gaps from secondary electrons of actuation gas and plasma electrons.

EFFECT: providing of high velocity of coating, ability to effect on coating features and increased adherence of coating to support.

SUBSTANCE: invention concerns coating field in vacuum. Particularly it concerns methods and facilities for coating on internal surface of odd-shaped details. Method includes rod-shaped cathode introduction into internal chamber of treated product, cathode is implemented of covering material, its fume and material vapor condensation on surface of treated detail. At that rod-shaped cathode is evaporated by cathode spots of vacuum arc, which are displaced on it butt surface by means of magnetic field through current contact jaw from nonretentive material. During the evaporation method rod-shaped electrode is introduces into detail till coincidental occurrence of its butt surface with pass border of detail diametrical surface to conical, then rod-shaped cathode is displaced backwards till overall derivation of it from treated detail. Facility contains rod-shaped cathode made of evaporated material, current contact jaw located coaxial to it, igniter electrode and solenoid for magnetic field creating. At that rod-shaped cathode is installed removable lengthwise of treated detail axis, current contact jaw which is anode is implemented from nonretentive material, at that part of current contact jaw distant from cathode is located in solenoid, axis of which coincides axis of treated detail.

EFFECT: providing of ability of coating on internal surfaces of details with small-bore chamber.

SUBSTANCE: invention relates to the technology of metallised material production for shielding from electromagnetic radiation in a broad range. Metallised material ''Nanotex'' is made of synthetic monofilament thread with diameter of 30-50 micron, and a number of threads is 30-160 threads per cm and surface density is 10-50 g/m2. Material has orifices between beam threads and shoots, size of which ranges within 1d-9d, where d is thread's diameter. Metal pads with predetermined surface resistance can be distributed over the material by weave or woven methods. The invention ensures production of the material with stable performances having high shielding capacity from different types of radiation including high-frequency radiation ranged from 300 to 16000 MHz.

EFFECT: production of the material with stable performance having high shielding capacity from different types of radiation.

SUBSTANCE: method includes forming of permeable skeleton structure from contacting fibres and their integration into entity using thermal processing up to diffusive penetration. After that, working element is coated with layer of aluminium 5÷12 μm thick using magnetron sputtering in vacuum by flat magnetron with disbalanced magnetic field. At least 95% aluminium is used as a target. Before coating, the surface of working element is activated using ionic source. After the coating, the working element undergoes homogenising annealing, until aluminium penetrates into the surface of working element on at least 1.5 μm.

SUBSTANCE: invention is related to methods of quasi-crystalline materials, particularly films of Al-Pd-Re, Al-Fe-Cu composition that might be used due to their unique qualities in bearings, applied as protective coatings in different fields of machine building, aircraft industry and reactor building. Layerwise application of materials is carried out by method of cathode spraying in Penning cell. Number of sections and materials of cell cathodes are selected in accordance with composition of quasi-crystalline film. Then protective coating AI2O3 is applied and vacuum annealing is carried out. Total thickness of quasi-crystalline film is formed at the account of thickness change and total quantity of applied layers. As materials that are applied together with aluminium, materials from the following groups are selected: Cu, Fe, Cr, Co, V, Ni, Ti, Mn, Pd, Ru, Re, Rh, Tr, Mn, Mo, Os, Si, Mg, Li.

FIELD: machine engineering, namely, manufacture of parts with coating with use of magnetron atomizer.

SUBSTANCE: target has outer and inner sides and it is made at least partially of atomized material. Magnets heat insulated relative to target are arranged at inner side of it. At least one pipeline through which cooling fluid is fed and which has portion of wall that does not transmit heat directly from target. Each magnet is mounted with possibility of changing distance from said portion of pipeline wall; between each magnet and respective portion of pipeline wall intermediate heat transfer member is arranged. Said member is made of non-ferromagnetic magnetic material with high heat conductance.

SUBSTANCE: method is realized due to magnetron spraying while supplying to target pulse bipolar voltage. Invention provides improved uniformity of parameters of film of oxide of zinc doped with aluminum at temperature of substrate no more than 150°C.

SUBSTANCE: device can be used for making items having coatings made of metals, glass, polymer films and fabrics. Anode of device has gas distribution system, which provides uniform supply of working gas along total surface of cathode to be sputtered; anode is under positive potential. Cathode has cooling system and cathode-target to be sputtered, which target-cathode is disposed between poles of magnetic system. Magnetic system has set of magnets with pole tips disposed onto water-cooled magnetic circuit made of soft magnetic steel. Set of magnets is under floating potential. Factor of usage of target material is equal to 60-70%.

FIELD: application of reinforcing, protective and decorative coats on articles in vacuum.

SUBSTANCE: proposed method includes electric arc spraying of cathode target and treatment of metal plasma flow in crossing electric and magnetic fields in cavity of additional anode of electric arc device. Dependent discharge of reaction and/or inert gas is ignited inside cavity of this additional anode. Metal plasma flow is additionally treated while passing through this discharge. Flow containing ions of gas and ions of material of cathode target settles on surface to be coated; potential of article is below potential of additional anode by 2000 V.